반응 #92989

반응 방정식

16β-ethyl-17β-bromoacetoxy-4-estren-3-one

4-methylvaleric acid

→

above-identified compound

16β-Ethyl-17β-(4-methylvaleryl)oxyacetoxy-4-estren-3-one

용매

acetone

NaOH

반응 조건

후처리

1. 1
   온도The mixture is refluxed for 6 hours
2. 2
   workup.DISTILLATIONThe acetone is distilled off under reduced pressure and 10 ml of water
3. 3
   workup.ADDITIONis added to the residue
4. 4
   추출followed by extraction with 100 ml of ethyl acetate
5. 5
   기타The organic layer is separated
6. 6
   세척washed with water and saturated aqueous sodium chloride solution
7. 7
   건조dried over anhydrous sodium sulfate
8. 8
   workup.DISTILLATIONThe solvent is then distilled off
9. 9
   세척the residue is subjected to column chromatography, elution
10. 10
    기타The eluate is evaporated under reduced pressure
11. 11
    기타to remove the solvent

실험 절차

In 35 ml of acetone is dissolved 1.0 ml of 4-methylvaleric acid, and 4.6 ml of 2N-NaOH and then 1.9 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are added to the above solution. The mixture is refluxed for 6 hours. The acetone is distilled off under reduced pressure and 10 ml of water is added to the residue, followed by extraction with 100 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is then distilled off and the residue is subjected to column chromatography, elution being carried out with 600 ml of diisopropyl ether-n-hexane (1:1). The eluate is evaporated under reduced pressure to remove the solvent, giving 1.3 g of the above-identified compound as a colorless viscous oil.

출처